CN103627612B - The white wine cold soaking of fragrant solomonseal rhizome polyoses, countercurrent extraction method and line Quality Control method thereof in wine-making technology - Google Patents
The white wine cold soaking of fragrant solomonseal rhizome polyoses, countercurrent extraction method and line Quality Control method thereof in wine-making technology Download PDFInfo
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Abstract
The white wine cold soaking of fragrant solomonseal rhizome polyoses, countercurrent extraction method and line Quality Control method thereof in wine-making technology.Extracting method: (1) radix polygonati officinalis is thinly sliced, or cut into chunks, or be broken into particle; (2) use the white wine of ethanol concn volume ratio 45%-55%, in mass ratio the feed ratio normal temperature cold soaking of 1:7.0-1:8.0; (3) use the white wine of ethanol concn volume ratio 45%-55%, countercurrent extraction.The radix polygonati officinalis of prioritization scheme is thinly sliced, or cuts into chunks, or flattens by external force after being broken into particle.The inventive method is direct, efficiency is high, avoids the difficulty of filtration; Evade the pollution suffering mould; The precipitation of polysaccharide in health promoting wine that molecular weight can be avoided excessive.For the ideal method that the radix polygonati officinalis in wine-making technology is extracted.The scheme of control method does not need the pre-treatment of sample; Analytical procedure is few, error effect factor is few; Consuming time short; The demand to batch samples Fast Measurement and line Quality Control can be met.
Description
Technical field
The present invention relates to a kind of extracting method, be specifically related to white wine cold soaking, the countercurrent extraction method of fragrant solomonseal rhizome polyoses in a kind of wine-making technology.The line Quality Control method of fragrant solomonseal rhizome polyoses white wine cold soaking, countercurrent extraction process in wine-making technology is also related in prioritization scheme of the present invention.
Background technology
Radix polygonati officinalis, for the dry rhizome of Liliaceae HUANGJING ZANYU CAPSULE radix polygonati officinalis (Polygonatum odoratum (Mill.) Druce), it is one of medicinal and edible Chinese medicine, record Chinese Pharmacopoeia 2010 editions [Chinese Pharmacopoeia Commission. Chinese Pharmacopoeia () [S]. Beijing: Chemical Industry Press, 2010].Radix polygonati officinalis taste is sweet, is slightly cold.There is nourishing YIN to relieve dryness, the merit promoted the production of body fluid to quench thirst, have hypoglycemic, antitumor, anti-oxidant isoreactivity.
Radix polygonati officinalis contains a large amount of polysaccharide, the compositions such as a small amount of steroidal saponin, flavones, and wherein polysaccharide is divided into again the oligosaccharides of molecular weight as radix polygonati officinalis Polylevulosan; The polysaccharide larger with molecular weight, as radix polygonati officinalis mucopolysaccharide.Radix polygonati officinalis Chinese liquor extraction liquid is in causing and the important intermediate of health promoting wine, is mainly molecular weight polysaccharide, radix polygonati officinalis oligosaccharides, and a small amount of radix polygonati officinalis saponin(e and flavone component.Document one reports that fragrant solomonseal rhizome polyoses has enhancing hypoxia tolerance (Sun Liyan; Liu Zhenliang; Sun Jinxia, etc. fragrant solomonseal rhizome polyoses is on the impact [J] of mouse oxygen deficit tolerance effect. Journal of Shandong agri.Univ: natural science edition, 2008; 39 (3): 335-338), anti-ageing (Dan Ying; Jiang Dong, Pan Xingyu, etc. fragrant solomonseal rhizome polyoses is on the impact [J] of Aging Mouse Modle immunologic function. Aged in China magazine; 2007,27 (1): 20-22. [5]; Dan Ying, Pan Xingyu, Jiang Dong, Deng. the antidotal experimental observation of fragrant solomonseal rhizome polyoses [J]. Chinese Clinical rehabilitation, 2006,10 (3): 79-81), anti-oxidant (Xu great Liang, Lin Hui, Li Shengqing, etc. the oxidation resistant experimental study in radix polygonati officinalis Aqueous extracts inside and outside [J]. Chinese medicinal materials, 2008,31 (5): 729-731), hypoglycemic (Ji Feng, Wei Xianyong, Liu Guanglong, etc. the experimental study [J] of fragrant solomonseal rhizome polyoses hypoglycemic activity. Jiangsu Chinese materia medica, 2006,27 (9): 70-71.) effect such as, therefore, exploitation fragrant solomonseal rhizome polyoses is significant.The extraction process of prior art fragrant solomonseal rhizome polyoses has some technical schemes, such as: China's No. 200910022946.7 application for a patent for invention, China's No. 200910012185.7 application for a patent for invention, China's No. 200410022863.5 application for a patent for invention, the method that above prior art extracts fragrant solomonseal rhizome polyoses is mostly water logging or poach, or increases the method such as supersound process, alcohol precipitation; These methods all need filtration to obtain product.
Prior art has following deficiency: (1), because the molecular weight of polysaccharide is far longer than Extraction solvent molecular weight, the viscosity of fragrant solomonseal rhizome polyoses is very large again, and the operation of the transfer processes such as filtration is very difficult; Filter material is often blocked, and cannot complete filtration procedure; In preparation transfer process, polysaccharide also very easily microbial contamination.(2) oligosaccharides of molecular weight is had in polysaccharide, as radix polygonati officinalis Polylevulosan; The polysaccharide larger with molecular weight, as radix polygonati officinalis mucopolysaccharide; The former is the important component in radix polygonati officinalis Chinese liquor extraction liquid, is also the important component as natural softening agent in wine; The latter often forms precipitation in white wine, brings threat to quality product, needs to evade removal part.
(3) polygonati rhizoma class medicinal material, elongated strip, bending, irregularity, diameter 2-8mm, quality is fine and close, and cause radix polygonati officinalis medicine materical crude slice to be amorphous cross-sectional slice, mostly be short cylinder, polysaccharide extract rate is subject to extreme influence, is often left in the basket.
(4) the online amount of radix polygonati officinalis Chinese liquor extraction liquid intermediate production process controls to continue to use polysaccharide determination method under Chinese Pharmacopoeia radix polygonati officinalis item always, and the online amount being difficult to meet online production controls.This measuring method complex pretreatment simultaneously; Analytical procedure is many, error effect factor many (as: precision adds the vitriol oil, phenol, shakes up, and process color heating is larger with the impact of cooling time); Length consuming time (each retinue typical curve 5 points), the more difficult demand met batch samples Fast Measurement and line Quality Control, also has no better fragrant solomonseal rhizome polyoses measuring method report so far.
In drinks making method, the method for composition near infrared spectrum on-line quick detection wine is adopted to report to some extent.Such as, China's No. 200810048945.5 application for a patent for invention, discloses the near infrared spectrum quick nondestructive online monitoring method of total flavones, total saponins in a kind of Traditional Chinese medicinal health-care wine (a kind of liquid system) production process; Comprise the following steps: (1). near infrared Monitoring systems is installed; (2). sampling determination chemical score; (3). set up the mathematical model of total flavones, total saponins material in the tested liquid of corresponding process point; (4). modelling verification and optimization; (5). total flavones, total saponin content in each process point liquid of on-line checkingi; (6). process monitoring and optimization.The method is by setting up the near infrared mathematical model of each process point index components of production process in advance, and this model is used for the quantitative analysis of index components in technological process, realize the line Quality Control to whole production process, good reproducibility of analysis results, quick nondestructive, relative deviation is less than 5%.
But the component total flavones that this patent adopts near infrared spectrum fast detection method to detect, total saponins are the compound of small-molecular-weight; And in causing and Chinese liquor extraction liquid be liquid system, the material of macromolecule is not only by fragrant solomonseal rhizome polyoses class material, and still form containing the material such as radix polygonati officinalis saponin(e and flavones chemical combination small molecules, completely different from the system of bibliographical information, have not yet to see fragrant solomonseal rhizome polyoses system in Chinese medicine, Rhizoma Polygonati Odorati extract system, the modeling rapid assay methods of radix polygonati officinalis Chinese liquor extraction liquid system or the online amount control method of production process.
Direct employing near infrared spectrum rapid detection polysaccharose substance, because the wide meeting of spectral coverage causes comprising lengthy and jumbled information, calculated amount and time also increase.Experiment shows: the near infrared spectrogram of the radix polygonati officinalis Chinese liquor extraction liquid of different batches is very similar, and overlapped, sets up the mathematical model of infrared data and chemical analysis data relation, and threshold is high, workload large, the research work that difficulty is large to be one.
The solvent direct extraction method of radix polygonati officinalis is there is not yet in prior art.Early-stage Study of the present invention shows: radix polygonati officinalis medicinal material quality is fine and close, glycosaminoglycan content is high, molecular weight is large, be unfavorable for that Extraction solvent spreads in medicinal material tissue, and polysaccharide molecular weight is far longer than Extraction solvent molecular weight in addition.Cause the extracting method of prior art not ideal enough.Polyose extraction process of the present invention is actual was divided into for 3 stages: (1) stage of soaking into is that white wine molecule infiltrates gradually, infiltrates in medicinal material tissue, and pre-stage test shows that radix polygonati officinalis quality is fine and close, and this stage is unusual; (2) swelling stage white wine molecule diffuses in polysaccharide molecule more further, makes the stage that polysaccharide is swelling, this process and temperature relation complexity even negative correlation; (3) dissolution phase polysaccharide is after certain hour is fully swelling, and polysaccharide diffuses in white wine more gradually.These 3 stages form complicated multifactor physical and chemical process, at this moment adopts cold soaking-heating countercurrent extraction method, can obtain required polysaccharide, take into account radix polygonati officinalis saponin(e flavone component.Therefore solvent direct extraction method of the present invention need overcome multifactorial interference perhaps, and selects conditions suitable, just can complete.
Owing to including the step of " when extracting solution polysaccharide concentration reaches 15-28mg/mL, stop extracting, collect extracting solution " in the present invention, so measure one of extracting solution polysaccharide concentration (online process quality control) content becoming this extracting method; Further optimization of the present invention (or completing second invention task of the application), relate to the line Quality Control method in the white wine cold soaking of fragrant solomonseal rhizome polyoses in wine-making technology, countercurrent extraction, it is characterized in that, step is as follows:
(1). the preparation of need testing solution:
In each process point, respectively get radix polygonati officinalis Chinese liquor extraction liquid respectively appropriate, wherein contain more than fragrant solomonseal rhizome polyoses concentration 8mg/mL in radix polygonati officinalis extracting solution; Centrifugally carry out solid-liquid separation, get supernatant liquor, with 0.05 micron of inorganic membrane filtration;
(2). gathered the near infrared spectrum of each process point need testing solution respectively by near infrared Monitoring systems after, carry out analytical calculation by corresponding near infrared mathematical model, namely draw fragrant solomonseal rhizome polyoses content in each process point liquid;
Described " gathering the near infrared spectrum of each process point need testing solution respectively " is the modeling of selection 6028.39 ~ 5943.53cm-1 wave band; Measuring parameter: transmission, resolving power 8cm-1, scanning times 64 times, sweep limit 4000 ~ 10000cm-1, each sample multiple scanning 3 times, is averaging spectrum; According to averaged spectrum, obtain polysaccharide content.
(3). detected data are passed through in process monitoring and optimization, determine the allotment data such as cold soaking time and adverse current temperature and time and monitor technique, adjust and optimize.
Described " corresponding near infrared mathematical model " refers to the model set up in accordance with the following methods:
A. the preparation of need testing solution:
In each process point, respectively get radix polygonati officinalis Chinese liquor extraction liquid respectively appropriate, wherein contain more than fragrant solomonseal rhizome polyoses concentration 8mg/mL in radix polygonati officinalis extracting solution; Centrifugally carry out solid-liquid separation, get supernatant liquor, with 0.05 micron of inorganic membrane filtration;
B. sampling determination chemical score gathers the liquid sample that each process point is no less than 30 different batches, and under using Chinese Pharmacopoeia radix polygonati officinalis item, method detects fragrant solomonseal rhizome polyoses content in mark extracting solution, obtains off-line index components chemical measurements;
C, set up the mathematical model of polysaccharide in the tested liquid of corresponding process point while carrying out second step operation, gather the near infrared spectrum of each process point liquid, and pre-treatment is carried out to each original spectrum, use chemo metric software, from above-mentioned corresponding spectrum, extract data message in mathematical operation mode, set up the mathematical model of relation between fragrant solomonseal rhizome polyoses content and absorption spectrum in tested liquid, described from above-mentioned corresponding spectrum, extract data message in mathematical operation mode and be: adopt the partial least square method (PLS) (PLS) in stoichiometry, combined by different filter method for de-noising and different model tuning methods, relation conefficient (R) relatively under different methods combination condition, correct square root of the variance (RMSEC), prediction square root of the variance (RMSEP), cross-validation square root of the variance (RMSECV) and because of subnumber (Factors), through repeatedly manually selecting and Integrated comparative, 1-Der+no smoothing is selected to extract feature, remove redundant information to greatest extent and eliminate the spectrum deviation that various interfering factors causes, set up quantitative calibration models.
D, the mathematical model that modelling verification uses oneself to set up with optimization carries out model prediction to the liquid sample that second step gathers, and contrasts with its chemical measurements, requires that error is less than 10%.
It is below the result of study to working mechanism of the present invention.
Fragrant solomonseal rhizome polyoses Chinese liquor extraction liquid prepared by cold soaking of the present invention+hot countercurrent extraction method is complex system, system composition is white wine, fragrant solomonseal rhizome polyoses, as radix polygonati officinalis Polylevulosan, radix polygonati officinalis saponin(e, flavone component, in this system, the molecular vibration spectrum of each composition is as shown near infrared collection of illustrative plates, and the frequency multiplication mostly being molecule because of absorption of vibrations behavior absorbs, and is difficult to describe by numeral and with the naked eye distinguish.But get this system liquid 1ml and add dehydrated alcohol 9ml, shake up, centrifugal, collecting precipitation, dry, fragrant solomonseal rhizome polyoses can be obtained, its molecular fingerprint feature, IR, KBr, v cm-1(T%): 3366.9 (19.1), 2933.7 (33.3), 2354.4 (83.96), 1736.3 (52.4), 1630.7 (37.87), 1417.4 (23.53), 1131.1 (13.31), 1023.3 (9.2), 930.2 (17.45), 814.4 (27.99), 595.6 (20.44).
1, medicinal material quality affects the impact of extraction yield.Radix polygonati officinalis medicinal material is difficult to pulverize, even if pulverize but caking in leaching process between fragment, causes sticky pot to be unfavorable for extracting and transfer.The present invention thinly slices radix polygonati officinalis medicine materical crude slice or is broken into particle, and then flatten further, extraction efficiency is greatly improved, thus addresses this problem.
Radix polygonati officinalis after flattening and broken radix polygonati officinalis, extracting polysaccharide content all increases with the increase of extraction time, but the polysaccharide content flattening radix polygonati officinalis is higher than the polysaccharide content of normal radix polygonati officinalis, flattens radix polygonati officinalis extraction yield high; But within 2 days, the highest extract concentration only has 13.48mg/mL, could not reach expection content.Along with time of repose extends, after 7 days, polysaccharide content obviously raises, and reaches 26.7mg/mL; Prompting this product fragrant solomonseal rhizome polyoses is oligosaccharides.Prompting this product fragrant solomonseal rhizome polyoses content and the cold soaking time closely related.
2, extraction time is on the impact of extraction yield.The present invention finds that polysaccharide wants first swelling, then dissolves, and needs to select right times, and B group (granular size 0.6-1cm) and extraction time positive correlation, have selected extraction conditions; A group (granular size 1-4cm) is poor with extraction time dependency, and extraction efficiency is poor.
3, extraction time, the impact of extract concentration extraction yield.Because the present invention finds that extracting polysaccharide has saturated phenomenon, when polysaccharide concentration reaches 10-15mg/mL and 20-25mg/mL, increasing time extracting concentration no longer increases or increases slowly; In addition, have oligosaccharides or the Polylevulosan of molecular weight in polysaccharide, the mucopolysaccharide that molecular weight is larger, in different concns alcohol, solubleness has gap, and 2 have competition dissolving relation, relevant with extraction time and extract concentration.
4, the alcohol number of degrees of medicine materical crude slice water content or white wine are on the impact of extractive content, discovery medicine materical crude slice water content or low ethanol concn white wine in the short period of time (several hours) have positive effect to extraction, but along with the prolongation of extracting, produce negative effect to extraction, comparative test result shows that medicine materical crude slice water content 10-15% extraction effect is better.
5, Extracting temperature, countercurrent extraction speed, medicinal material water content on the impact of extraction yield, thin slice and/or flatten and Extracting temperature and time positive correlation, but macrobead (being greater than 1-4cm) and Extracting temperature and temporal correlation poor, extraction efficiency is low.
6, near-infrared model is established in above prioritization scheme, can be used for the online process quality control of radix polygonati officinalis extracting solution complex system, be applicable to assay and the line Quality Control of batch samples, the quality monitoring for radix polygonati officinalis Chinese liquor extraction liquid provides a kind of new method and thinking.
PLS main cause subnumber used because of subnumber very few, in spectrum, some useful informations cause the predictive ability of model poor because of not involved; Otherwise, selection because of subnumber too much, then occur that Expired Drugs affects its result.Fig. 2 is main cause subnumber Factor, RMSECV, predictive residual error sum of squares (PRESS) correlogram, adopts internal verification method, according to the change of cross-validation square root of the variance (RMSECV) with main cause subnumber.
Below the demonstration to this detection method:
1. measurement of the polysaccharide content
The preparation of 1.1 reference substance solution, the drafting of typical curve are all by radix polygonati officinalis polysaccharide from medicinal materials content assaying method
[1].
The preparation of 1.2 need testing solutions and assay
Improve slightly by Chinese Pharmacopoeia method, get radix polygonati officinalis Chinese liquor extraction liquid appropriate (about 4ml), put in 5ml centrifuge tube, centrifugal 10min, precision gets supernatant liquor 1ml, puts in 10ml centrifuge tube, add 95% ethanol 8ml, shake up, centrifugal 10min, incline supernatant liquor, add water, ultrasonic dissolution precipitates, and quantitatively transfers in 100ml measuring bottle, add water, be settled to scale.Precision measures 2ml, puts in 10ml volumetric flask, adds water and be settled to scale, shake up, obtain need testing solution.
Precision measures need testing solution 2ml, put in tool plug test tube, precision adds 4% phenol 1ml, mixing, rapid precision adds vitriol oil 7ml, abundant mixing, in 40 DEG C of insulation 30min, takes out, ice bath 5min, survey its absorbance (A) at 490nm wavelength place, with typical curve calculating concentration (C) under 2.1.1 item, 73 batches of radix polygonati officinalis Chinese liquor extraction liquid polysaccharide contents are 3.47 ~ 15.78mg ﹒ mL
﹣ 1.
The collection of 2 near infrared spectrum data
By centrifugal for 73 parts of sample liquid, get appropriate in liquid-like QC, measuring parameter: transmission, resolving power 8cm
-1, scanning times 64 times, sweep limit 4000 ~ 10000cm
-1, each sample multiple scanning 3 times, is averaging spectrum.Fig. 1 is shown in 73 parts of radix polygonati officinalis Chinese liquor extraction liquid near infrared spectrum superpositions.
The method of 3 Modling model
By radix polygonati officinalis Chinese liquor extraction liquid polysaccharide content value and near infrared spectrum input TQ Analyst quantitative analysis software, carry out data processing, adopt the partial least square method (PLS) (PLS) in stoichiometry to set up quantitative calibration models.Combined by different filter method for de-noising and different model tuning methods, relation conefficient (R) relatively under different methods combination condition, correct square root of the variance (RMSEC), prediction square root of the variance (RMSEP), cross-validation square root of the variance (RMSECV) and because of subnumber (Factors), the results are shown in Table 1.Through repeatedly manually selecting and Integrated comparative, final 1-Der+no smoothing treatment effect of selecting is best.
The comparison of table 1 polysaccharide model different pretreatments method
| Pretreatment process | R | RMSEC | RMSEP | RMSECV | Factors |
| Original spectrum | 0.9797 | 0.638 | 0.583 | 0.808 | 6 |
| 1-Der+no smoothing | 0.9833 | 0.579 | 0.624 | 0.771 | 6 |
| 1-Der+SG | 0.9803 | 0.629 | 0.717 | 0.802 | 6 |
| 2-Der+no smoothing | 0.8837 | 1.49 | 2.30 | 2.28 | 6 |
| 2-Der+SG | 0.9099 | 1.32 | 1.34 | 1.62 | 5 |
| 2-Der+Norris | 0.9385 | 1.10 | 1.35 | 1.26 | 4 |
The selection of 3.1 modeling spectral coverages
With relation conefficient (R) with correct square root of the variance (RMSECV) for index, by TQ Analyst software recommend, final radix polygonati officinalis base wine extraction liquid selects 6028.39 ~ 5943.53cm
-1wave band modeling.
3.2 because of subnumber selection
During Modling model, selected main cause subnumber is relatively large on the impact predicted the outcome.If PLS used because of subnumber very few, in spectrum, some useful informations cause the predictive ability of model poor because of not involved; Otherwise, selection because of subnumber too much, then occur that Expired Drugs affects its result.Fig. 2 is main cause subnumber Factor, RMSECV, predictive residual error sum of squares (PRESS) correlogram, and adopt internal verification method, according to the change of cross-validation square root of the variance (RMSECV) with main cause subnumber, main cause subnumber is chosen as 6.
The foundation of 3.3 models
From sample, choose 58 for standard samples collection, 15 is checking collection, optimizes, pick out overflow value, to ensure the accuracy of model through Outliers.Use PLS method to set up the quantitative calibration models of radix polygonati officinalis Chinese liquor extraction liquid polysaccharide, modeling factors number is 6.As shown in Figure 3, coefficient R is 0.9703, RMSECV is 0.771 to result.
3.4 external certificate
Use the best calibration model set up, the polysaccharide content in forecast set is predicted.Polysaccharide predict the outcome in table 2, setting up regression equation between predictor and measured value is Y=0.8953X+1.215, R
2=0.9692.As shown in Table 2, the average relative error of predictor is 5.49%, therefore, can think that this calibration model is reliable.
Table 2 radix polygonati officinalis Chinese liquor extraction liquid external certificate result
4 conclusions
This experiment adopts near infrared spectroscopy, stechiometry, partial least square method (PLS) to establish radix polygonati officinalis Chinese liquor extraction liquid polysaccharide content model, this model has good predictive ability to polysaccharide content, the line Quality Control of production process can be met, realize quick, the harmless quantitative analysis of polysaccharide.
5 discuss:
5.1 PLS methods can adopt full spectral coverage to carry out modeling, but the wide meeting of spectral coverage causes comprising lengthy and jumbled information, and calculated amount and time also increase.Therefore, the prediction accuracy in order to improve model can carry out the optimization of spectral coverage.Show that the radix polygonati officinalis Chinese liquor extraction liquid near infrared spectrogram of different batches is very similar in Fig. 1 herein, and overlapped.Therefore the dependency between polysaccharide total amount and individual wavelengths point absorbancy cannot be judged according to this figure, chemometrics method must be utilized in certain wave band, set up its mathematical model, the relation between polysaccharide total amount and spectrum could be determined.
5.2 traditional Analysis of polysaccharides methods are loaded down with trivial details, this experimental technique does not need the pre-treatment of sample, scanning near infrared spectrum substitutes into model just can obtain polysaccharide content, and be applicable to assay and the line Quality Control of batch samples, the quality monitoring for radix polygonati officinalis Chinese liquor extraction liquid provides a kind of new method and thinking.
Be below brief summary of the present invention:
White wine cold soaking, the countercurrent extraction method of fragrant solomonseal rhizome polyoses in wine-making technology: (1). white wine is middle white wine of making peace, and with Chinese sorghum for wanting raw material, brewages with Thousand Islands lake water.(2). radix polygonati officinalis is broken into broken particle, and 1. breaking feature for shred or to be ground into particle, and size is about 0.1-0.3cm; 2. segment becomes to be about 0.6-1cm, flattens; (3). with in causing and white wine, ethanol concn 45%-55%(v/v), by radix polygonati officinalis: white wine=1:7.0-1:8.0 (w/w) feeds intake, normal temperature cold soaking+heating countercurrent extraction, extracting solution is got in collection, and wherein, normal temperature refers to production site temperature, heating adverse current temperature is 30-80 DEG C, the circulated in countercurrent speed 1.0-1.5T/h*5kg of every 5kg medicinal material; (4). normal temperature cold soaking+heating countercurrent extraction step can hocket.In prioritization scheme, broken radix polygonati officinalis becomes small-particle, then flattens by external force.Its water content control is at mass ratio 10-15%.Further optimization is the white wine cold soaking of fragrant solomonseal rhizome polyoses in wine-making technology, the online amount of heating countercurrent extraction process controls, it is characterized in that the process of modeling, according to the extracting solution of online acquisition, direct Quick Acquisition near infrared spectrum, substitutes in model and obtains polysaccharide content.A kind of ideal extracting method and the online amount control method of production process are provided.
Compared with prior art, the present invention has obvious advantage: method of the present invention is direct, efficiency is high, does not need to filter, and avoids the difficulty of filter operation; Evade the operation link that polysaccharide suffers mould contamination; The precipitation of polysaccharide in health promoting wine that molecular weight is larger can be avoided simultaneously.For the radix polygonati officinalis Chinese liquor extraction liquid in wine-making technology provides a kind of ideal preparation method.Prioritization scheme of the present invention overcomes many deficiencies of the online amount control method of existing radix polygonati officinalis white wine, does not need the pre-treatment of sample; Analytical procedure is few, error effect factor is few; Consuming time short; The demand to batch samples Fast Measurement and line Quality Control can be met.
Summary of the invention
In order to overcome the above-mentioned deficiency of prior art, the invention provides white wine cold soaking, the countercurrent extraction method of fragrant solomonseal rhizome polyoses in a kind of wine-making technology, the method is direct, efficiency is high, does not need to filter, and avoids the difficulty of filter operation; Evade the operation link that polysaccharide suffers mould contamination; The precipitation of large molecular weight polysaccharides in health promoting wine can be avoided simultaneously.For the radix polygonati officinalis Chinese liquor extraction liquid in wine-making technology provides a kind of ideal preparation method.Online amount control method when fragrant solomonseal rhizome polyoses white wine cold soaking, countercurrent extraction in wine-making technology is also related in prioritization scheme of the present invention.Prioritization scheme will overcome many deficiencies of the online amount control method of prior art radix polygonati officinalis white wine, a kind of online amount control method is newly provided, be the near infrared spectroscopy of polysaccharide content in a kind of rapid detection radix polygonati officinalis Chinese liquor extraction liquid, the method does not need the pre-treatment of sample; Analytical procedure is few, error effect factor is few; Consuming time short; The demand to batch samples Fast Measurement and line Quality Control can be met.
The technical scheme completing foregoing invention task is: white wine cold soaking, the countercurrent extraction method of fragrant solomonseal rhizome polyoses in a kind of wine-making technology, and it is characterized in that, step is as follows:
(1). radix polygonati officinalis is thinly sliced, and cuts into chunks, or is broken into particle;
. use ethanol concn 45%-55%(v/v) white wine, by feed ratio (mass ratio) the normal temperature cold soaking of 1:7.0-1:8.0;
. use ethanol concn 45%-55%(v/v) white wine, countercurrent extraction.
Described " ethanol concn 45%-55%(v/v) white wine ", during the present invention recommends employing to cause and white wine.
Wherein, step normal temperature (2) refers to the temperature of production site.Can be different with the difference in season.
The present invention has following prioritization scheme:
1, described " radix polygonati officinalis is thinly sliced ", refers to the thin slice being cut into thickness 0.1-0.3cm; " cut into chunks " and refer to and be cut into the long section of 0.6-1cm; " be broken into particle " and refer to the particle being broken into size 0.6-1cm;
Described " being broken into particle " can not be broken into very thin fine powder, phenomenon that fine powder easily occurs " knot crispy rice ", is unfavorable for that solvent infiltrates, swelling, the dissolving of polysaccharide, is namely unfavorable for the extraction efficiency of polysaccharide.
2, increase and have following steps: after (1)-1 radix polygonati officinalis is thinly sliced or is broken into particle, flatten by external force.
Because when thinly slicing or be broken into particle, only have the radix polygonati officinalis part cell of incision to be cut open, and majority of plant cell is complete, is unfavorable for the stripping of polysaccharide; And when flattening further, majority of plant cell is destroyed, cell wall rupture, is conducive to the stripping of polysaccharide;
3, described step " radix polygonati officinalis is thinly sliced or is broken into particle " (1), its water content control is at mass ratio 8%-15%; The water content that the application recommends is 13%;
4, the volume ratio of described step white wine (2) recommends employing 50%; By 1:6-9(mass ratio) feed ratio normal temperature cold soaking;
5, the time of described step use volume ratio white wine normal temperature cold soaking is (2) more than 12 hours.
In method of the present invention, the cold soaking time is very important.Described " time of cold soaking is more than 12 hours " refers to, thinner thin slice or less particle, cold soaking 12 hours-8 days, thicker thin slice or larger particle, and cold soaking is also passable for January.The time longer leaching effect of cold soaking is better, but the production cycle can be made long.The present invention advises cold soaking 24 hours-168 hours; Preferably 24 hours-72 hours; Recommend employing 72 hours;
6, described step (3) use ethanol concn 45%-55%(v/v) white wine, during countercurrent extraction, be heated to 30-80 DEG C, recommend 50-70 DEG C; Preferred 65-70 DEG C;
7, during described step countercurrent extraction (3), the every 5 kilograms of medicinal materials of circulated in countercurrent speed are 1.0-1.5T/h*5kg(ton/hour * 5 kilograms of medicinal materials);
8, the described step countercurrent extraction time is (3) about 6-8h; Or when extracting solution polysaccharide concentration reaches 15-28mg/mL, stop extracting, collect extracting solution;
The application recommends, and when extracting solution polysaccharide concentration reaches 15-20mg/mL, stops extracting, collects extracting solution.
9, increase has following steps:
(4), (5): repeating step (2)-step (3); That is, above step (2), (3) extracting method repeat twice, or step (2)-(3) step hocket for several times (normal temperature cold soaking+heating countercurrent extraction step can hocket), extraction time 2-8 days, cold soaking and countercurrent extraction time are than 2:1 – 8:1;
(6). merge twice or extracting solution for several times, place for subsequent use;
(7). before use, by the extracting solution diatomite filtration after merging, blend by given process.
In primary extracting solution, micromolecular polysaccharide is more; In secondary extracting solution, macromolecular polysaccharide is more.Merge the extracting solution of twice and after placing for some time, due to the Competition of solubleness, the more macromolecular polysaccharide of part can be separated out, and is conducive to improving the quality of extracting solution.
Accompanying drawing explanation
Fig. 1 is in of the present invention causing and white wine polyoses extract Fourier IR spectrogram;
Fig. 2 is in of the present invention causing and the nearly IR spectrogram of Chinese liquor extraction liquid;
Fig. 3 is the dependency of polygonatum liquor base extracting solution online quantitatively IR model prediction result and off-line chemical assay result;
Fig. 4 is the authentication result figure of the online quantitatively IR model of calibration set Factor, RMSECV, PRESS.
Embodiment
Embodiment 1, gets radix polygonati officinalis medicine materical crude slice appropriate, is broken into particle 0.1-0.3cm, add 50 degree of white wine respectively by the feed ratio of 1:7.5, cold soaking spends the night, temperature 50-70 DEG C of countercurrent extraction (circulated in countercurrent speed 1.0T/h*5kg) about 6-8h, collect extracting solution, as extracting solution-1, for subsequent use, add 50 degree of white wine with method second time, within cold soaking 16-64 hour, (advise Friday, Saturday, amount to 3 days Sunday), daytime, countercurrent extraction (circulated in countercurrent speed 1.0T/h) about 6-8h, collected extracting solution-2, for subsequent use.Merge No. 2 extracting solutions 1 and 2, as storing solution, place for subsequent use, use front diatomite filtration, blend by given process.
Embodiment 2,
Get radix polygonati officinalis medicine materical crude slice appropriate, broken or be cut into 0.6-1cm particle, flatten, or be cut into 0.6-1cm particle again after flattening, 50 degree of white wine are added respectively by the feed ratio of 1:7.5, cold soaking temperature: place temperature 10-35 degree, heating adverse current temperature: 50-70 DEG C, circulated in countercurrent speed 1.0T/h, cold soaking+countercurrent extraction time is 24-72 hour, " cold soaking-adverse current-cold soaking-adverse current " interval is carried out, the cold soaking time: heating adverse current time=2:1 ~ 8:1, extracting solution-1 is got in collection, for subsequent use, 50 degree of white wine are added with method second time, " cold soaking-adverse current-cold soaking-adverse current " hocket extraction, extracting solution-2 is got in collection, for subsequent use.Merge No. 2 extracting solutions, as storing solution, place for subsequent use, use front diatomite filtration, blend by given process.
Get radix polygonati officinalis extracting solution appropriate (about 4ml) respectively, centrifugal 10min in 5ml centrifuge tube; Get the above-mentioned centrifuged supernatant of 1ml in 10ml centrifuge tube, add 8ml ethanol, shake up, centrifugal 10 minutes; Polysaccharide is measured by drafting method.The results are shown in Table 1,2.
Process results shows that the 1st cold soaking effect is better, and extract concentration is 18.6mg/mL, and the 2nd time cold soaking effect is general, and extract concentration is 4.77mg/mL, is only the 1st time 25%; 3rd cold soaking effect is poor is 2.78mg/mL, is only the 1st time 15%; Therefore, select second extraction method, the accumulative content that extracts can reach 25.77mg/mL, meets the requirements.
Embodiment 3,
Get radix polygonati officinalis medicine materical crude slice appropriate, be broken into small-particle 0.1-0.3cm, or flatten after being cut into 0.6-1cm particle, or be cut into 0.6-1cm particle after flattening, add 50 degree of white wine respectively by the feed ratio of 1:7.5, cold soaking spends the night 16h, daytime, normal temperature countercurrent extraction was about 6-8h, extracted 2 days, collected and got extracting solution-1, for subsequent use, add 50 degree of white wine with method second time, cold soaking spends the night, and (the suggestion time can extend to 3 days, namely, utilize Friday, Saturday, Sunday leaves standstill), daytime, normal temperature countercurrent extraction was about 6-8h, extracting solution-2 is got in collection, for subsequent use.Blend (noticing that radix polygonati officinalis volume adds 1 times) by given process.
Embodiment 4,
2.1 get radix polygonati officinalis medicine materical crude slice in right amount, are cut into 0.6-1cm, flatten, add 50 degree of white wine respectively by the feed ratio of 1:7.5, cold soaking spends the night, temperature 50-70 DEG C of countercurrent extraction (circulated in countercurrent speed 1.0T/h) about 6-8h, extracting solution-1 is got in collection, for subsequent use, adds 50 degree of white wine with method second time, cold soaking (advises Friday mistake-night, Saturday, amount to 3 days Sunday), daytime countercurrent extraction (circulated in countercurrent speed 1.0T/h) about 6-8h, extracting solution-2 is got in collection, for subsequent use.Merge No. 2 extracting solutions, place for subsequent use, use front diatomite filtration, blend by given process.
2.2(and 2.1 is not both, and go to pieces 0.1-0.3cm) get radix polygonati officinalis medicine materical crude slice in right amount, go to pieces 0.1-0.3cm, and the same method is extracted.
2.3(and 2.1 is not both, and cold soaking and countercurrent extraction time respectively increase 2-3 doubly) to get radix polygonati officinalis medicine materical crude slice appropriate, thinly slice 0.6-1cm, flatten, by 1:7.5, feed ratio add 50 degree of white wine respectively, cold soaking 32-48 hour, temperature 65-70 DEG C countercurrent extraction (circulated in countercurrent speed 1.0T/h) about 16-24h, extracting solution-1 is got in collection, for subsequent use, add 50 degree of white wine, cold soaking-sky countercurrent extraction with method second time, extracting solution-2 is got in collection, for subsequent use.Merge No. 2 extracting solutions, place for subsequent use, use front diatomite filtration, blend by given process.
2.4(and 2.1 is not both, and does not flatten, and all the other are with 2.3) to get radix polygonati officinalis medicine materical crude slice appropriate, thinly slice 0.6-1cm, by 1:7.5, feed ratio add 50 degree of white wine respectively, cold soaking 32-48 hour, temperature 65-70 DEG C of countercurrent extraction (circulated in countercurrent speed 1.0T/h) about 16-24h, collects and gets extracting solution-1, for subsequent use, 50 degree of white wine are added with method second time, cold soaking-sky countercurrent extraction, collects and gets extracting solution-2, for subsequent use.Merge No. 2 extracting solutions, place for subsequent use, use front diatomite filtration, blend by given process.
2.6(and 2.1 is not both, and countercurrent extraction temperature is 30-50 DEG C)
Get radix polygonati officinalis medicine materical crude slice appropriate, be cut into 0.6-1cm, flatten, add 50 degree of white wine respectively by the feed ratio of 1:7.5, cold soaking spends the night, 30-50 DEG C of countercurrent extraction (circulated in countercurrent speed 1.0T/h) about 6-8h, extracting solution-1 is got in collection, for subsequent use, adds 50 degree of white wine with method second time, cold soaking (advises Friday mistake-night, Saturday, amount to 3 days Sunday), daytime 30-50 DEG C of countercurrent extraction (circulated in countercurrent speed 1.0T/h) about 6-8h, extracting solution-2 is got in collection, for subsequent use.Merge No. 2 extracting solutions, place for subsequent use, use front diatomite filtration, blend by given process.
2.5(and 2.1 is not both, do not flatten, countercurrent extraction, temperature is 30-50 DEG C, time lengthening is to 13-16h) to get radix polygonati officinalis medicine materical crude slice appropriate, thinly slice, 0.6-1cm, 50 degree of white wine are added respectively by the feed ratio of 1:7.5, cold soaking spends the night, temperature 50-70 DEG C of countercurrent extraction is about 16h, circulated in countercurrent speed 1.0T/h, extracting solution-1 is got in collection, for subsequent use, 50 degree of white wine are added with method second time, cold soaking spends the night (advises Friday, Saturday, amount to 3 days Sunday to spend the night), daytime countercurrent extraction (circulated in countercurrent speed 1.0T/h) about 13-16h, extracting solution-2 is got in collection, for subsequent use.Merge No. 2 extracting solutions, place for subsequent use, use front diatomite filtration, blend by given process.
Table 1 measurement result
；
Table 2 measurement result (according to upper table, accumulation result)
Embodiment 5, substantially identical with above embodiment, but use the white wine of ethanol concn 45% instead, by feed ratio (mass ratio) the normal temperature cold soaking of 1:7.0; The time of cold soaking is 72 hours; By the white wine countercurrent extraction of ethanol concn 45%.The white wine cold soaking of described step use ethanol concn 45% (3), reheats 50 DEG C of countercurrent extraction.
Embodiment 6, substantially identical with above embodiment, but use the white wine of ethanol concn 55% instead, by feed ratio (mass ratio) the normal temperature cold soaking of 1:8.0; The time of cold soaking is 24-72 hours; By the white wine liquid countercurrent extraction of ethanol concn 55%.During the white wine countercurrent extraction of described step use ethanol concn 55% (3), be heated to 70 DEG C.
Embodiment 7, substantially identical with above embodiment, but described " radix polygonati officinalis is thinly sliced ", refer to the particle or thin slice that are broken into size 0.6-1cm.Do not flatten after section, directly with in causing and white wine, ethanol concn 45%-55%(v/v), normal temperature cold soaking.The time of cold soaking is 168 hours.Described step (3) with white wine countercurrent extraction time, be heated to 30 DEG C.
Embodiment 8, substantially identical with above embodiment, but described " radix polygonati officinalis is thinly sliced " its water content control is at mass ratio 8%.(2) described step is 12 hours with the time of the white wine normal temperature cold soaking of ethanol concn 55%.Described step (3) with white wine countercurrent extraction time, be heated to 80 DEG C.
Embodiment 9, substantially identical with above embodiment, but described " radix polygonati officinalis is thinly sliced " its water content control is at mass ratio 15%.Described step (2) be 1 week with the time of white wine normal temperature cold soaking.
Embodiment 10, substantially identical with above embodiment, substantially identical with above embodiment, but, described step (2) be cold soaking 24 hours with the time of white wine normal temperature cold soaking; When (3) described step uses white wine countercurrent extraction, be heated to 60 DEG C.
Embodiment 11, substantially identical with above embodiment, but when (3) described step uses white wine countercurrent extraction, be heated to 65 DEG C.
Water content control is at mass ratio 8%-15%; The volume ratio of described step white wine (2) adopts 50%; The feed ratio normal temperature cold soaking of 1:6-9 in mass ratio; Described step use white wine (3), during countercurrent extraction, is heated to 70 DEG C; When extracting solution polysaccharide concentration reaches 15-20mg/mL, stop extracting, collect extracting solution.
Embodiment 12, substantially identical with above embodiment, but described step use white wine (3), during countercurrent extraction, be heated to 65-70 DEG C.
Meanwhile, increase has following steps:
(4), (5): repeating step (2)-step (3); Or step (2)-(3) step hockets for several times, extraction time 2-8 days, cold soaking and countercurrent extraction time are than 2:1 – 8:1.
Described step white wine cold soaking and countercurrent extraction time 2-8 days, cold soaking and countercurrent extraction time are than 2:1 – 8:1;
Embodiment 13, in extracting solution prepared by above-described embodiment either method, gets 3 lot numbers at random, centrifugal respectively, draw 1ml and add dehydrated alcohol 9ml, shake up, centrifugal, collecting precipitation, dry, obtain fragrant solomonseal rhizome polyoses, KBr: trial-product prepared by sample (1:50, w/w), compressing tablet, its spectrogram is gathered, trial-product IR molecular fingerprint feature, KBrv cm with FIR instrument
-1(T%): 3366.9 (19.1), 2933.7 (33.3), 2354.4 (83.96), 1736.3 (52.4), 1630.7 (37.87), 1417.4 (23.53), 1131.1 (13.31), 1023.3 (9.2), 930.2 (17.45), 814.4 (27.99), 595.6 (20.44).Similarity more than 98% between 3 batches.
Wherein, line Quality Control method, step is as follows:
(1). the preparation of need testing solution:
In each process point, respectively get radix polygonati officinalis Chinese liquor extraction liquid respectively appropriate, wherein contain more than fragrant solomonseal rhizome polyoses concentration 8mg/mL in radix polygonati officinalis extracting solution; Centrifugally carry out solid-liquid separation, get supernatant liquor, with 0.05 micron of inorganic membrane filtration;
(2). gathered the near infrared spectrum of each process point need testing solution respectively by near infrared Monitoring systems after, carry out analytical calculation by corresponding near infrared mathematical model, namely draw fragrant solomonseal rhizome polyoses content in each process point liquid;
Described " gathering the near infrared spectrum of each process point need testing solution respectively " is the modeling of selection 6028.39 ~ 5943.53cm-1 wave band; Measuring parameter: transmission, resolving power 8cm-1, scanning times 64 times, sweep limit 4000 ~ 10000cm-1, each sample multiple scanning 3 times, is averaging spectrum; According to averaged spectrum, obtain polysaccharide content.
(3). detected data are passed through in process monitoring and optimization, determine the allotment data such as cold soaking time and adverse current temperature and time and monitor technique, adjust and optimize.
Claims (9)
1. white wine cold soaking, the countercurrent extraction method of fragrant solomonseal rhizome polyoses in wine-making technology, it is characterized in that, step is as follows:
(1). radix polygonati officinalis is thinly sliced, or cuts into chunks, or is broken into particle;
(2). with the white wine of ethanol concn volume ratio 45%-55%, the feed ratio normal temperature cold soaking of 1:7.0-1:8.0 in mass ratio;
(3). with the white wine of ethanol concn volume ratio 45%-55%, countercurrent extraction;
Described step " radix polygonati officinalis is thinly sliced, or cuts into chunks, or is broken into particle " (1), its water content control is at mass ratio 8%-15%;
The volume ratio of described step white wine (2) adopts 50% ethanol concn; The feed ratio normal temperature cold soaking of 1:7.0-1:8.0 in mass ratio;
Described step (2) be more than 12 hours with the time of white wine normal temperature cold soaking;
Described step (3) with white wine countercurrent extraction time, be heated to 30-80 DEG C;
During described step countercurrent extraction (3), circulated in countercurrent speed is 1.0-1.5T/h*5kg;
Described step countercurrent extraction time 6-8h (3); Or when extracting solution polysaccharide concentration reaches 15-28mg/mL, stop extracting, collect extracting solution.
2. white wine cold soaking, the countercurrent extraction method of fragrant solomonseal rhizome polyoses in wine-making technology according to claim 1, it is characterized in that, described " radix polygonati officinalis is thinly sliced, or cuts into chunks, or is broken into particle ", refers to the thin slice being cut into thickness 0.1-0.3cm; Or be cut into the long section of 0.6-1cm, or be broken into the particle of size 0.6-1cm.
3. white wine cold soaking, the countercurrent extraction method of fragrant solomonseal rhizome polyoses in wine-making technology according to claim 1, is characterized in that, increases and has following steps: (1)-1 radix polygonati officinalis is thinly sliced, or cuts into chunks, or after being broken into particle, flattens by external force.
4. white wine cold soaking, the countercurrent extraction method of fragrant solomonseal rhizome polyoses in wine-making technology according to claim 1, it is characterized in that, the polysaccharide extracted is oligosaccharides, is characterized as the polysaccharide that the parameter in following table limits:
Table: fragrant solomonseal rhizome polyoses, FIR characteristic spectrum (KBr, υ cm
-1)
5. white wine cold soaking, the countercurrent extraction method of fragrant solomonseal rhizome polyoses in wine-making technology according to claim 4, is characterized in that,
Described step " radix polygonati officinalis is thinly sliced, or cuts into chunks, or is broken into particle " (1), its water content control is at mass ratio 13%;
Described step (2) be 12 hours-8 days with the time of white wine normal temperature cold soaking;
Described step use white wine (3), during countercurrent extraction, is heated to 50-70 DEG C;
Described step countercurrent extraction is (3) when extracting solution polysaccharide concentration reaches 15-20mg/mL, stops extracting, and collects extracting solution.
6. white wine cold soaking, the countercurrent extraction method of fragrant solomonseal rhizome polyoses in wine-making technology according to claim 5, is characterized in that,
Described step (2) be cold soaking 24 hours-168 hours with the time of white wine normal temperature cold soaking;
Described step use white wine (3), during countercurrent extraction, is heated to 65-70 DEG C.
7. according to white wine cold soaking, the countercurrent extraction method of fragrant solomonseal rhizome polyoses in the wine-making technology one of claim 1-6 Suo Shu, it is characterized in that, increase and have following steps:
(4), (5): repeating step (2)-step (3); Or step (2)-(3) step hockets for several times, extraction time 2-8 days, cold soaking and countercurrent extraction time are than 2:1 – 8:1;
(6). merge twice or extracting solution for several times, place for subsequent use;
(7). before use, by the extracting solution diatomite filtration after merging, blend by given process.
8. the online quality monitoring in wine-making technology described in claim 1 in the white wine cold soaking of fragrant solomonseal rhizome polyoses, countercurrent extraction method and the method for technique adjustment, it is characterized in that, step is as follows:
(1). the preparation of need testing solution:
In each process point, get radix polygonati officinalis Chinese liquor extraction liquid respectively appropriate, wherein contain more than fragrant solomonseal rhizome polyoses concentration 6mg/mL in radix polygonati officinalis extracting solution; Centrifugally carry out solid-liquid separation, get supernatant liquor, with 0.05 micron of inorganic membrane filtration;
(2). gathered the near infrared spectrum of each process point need testing solution respectively by near infrared Monitoring systems after, carry out analytical calculation by corresponding near infrared mathematical model, namely draw fragrant solomonseal rhizome polyoses content in each process point liquid;
Described " gathering the near infrared spectrum of each process point need testing solution respectively " is the modeling of selection 6028 ~ 5943cm-1 wave band; Measuring parameter: transmission, resolving power 8cm-1, scanning times 64 times, sweep limit 4000 ~ 10000cm-1, each sample multiple scanning 3 times, is averaging spectrum; According to averaged spectrum, obtain polysaccharide content;
(3). process monitoring and optimize and pass through detected data, determine allotment cold soaking time and adverse current temperature and time data technique is monitored, adjust and optimizes.
9. the online quality monitoring in wine-making technology according to claim 8 in the white wine cold soaking of fragrant solomonseal rhizome polyoses, countercurrent extraction method and the method for technique adjustment, it is characterized in that, described " corresponding near infrared mathematical model " refers to the model set up in accordance with the following methods:
A. the preparation of need testing solution:
In each process point, respectively get radix polygonati officinalis Chinese liquor extraction liquid respectively appropriate, wherein contain more than fragrant solomonseal rhizome polyoses concentration 8mg/mL in radix polygonati officinalis extracting solution; Centrifugally carry out solid-liquid separation, get supernatant liquor, with 0.05 micron of inorganic membrane filtration;
B. sampling determination chemical score gathers the liquid sample that each process point is no less than 30 different batches, and under using Chinese Pharmacopoeia radix polygonati officinalis item, method detects fragrant solomonseal rhizome polyoses content in mark extracting solution, obtains off-line index components chemical measurements;
C, set up the mathematical model of polysaccharide in the tested liquid of corresponding process point while carrying out second step operation, gather the near infrared spectrum of each process point liquid, and pre-treatment is carried out to each original spectrum, use chemo metric software, from above-mentioned corresponding spectrum, extract data message in mathematical operation mode, set up the mathematical model of relation between fragrant solomonseal rhizome polyoses content and absorption spectrum in tested liquid;
Described from above-mentioned corresponding spectrum, extract data message in mathematical operation mode and be: adopt the partial least square method (PLS) in stoichiometry, combined by different filter method for de-noising and different model tuning methods, relation conefficient relatively under different methods combination condition, correct square root of the variance, prediction square root of the variance, cross-validation square root of the variance and because of subnumber, through repeatedly manually selecting and Integrated comparative, 1-Der+no smoothing is selected to extract feature, remove redundant information to greatest extent and eliminate the spectrum deviation that various interfering factors causes, set up quantitative calibration models,
D, the mathematical model that modelling verification uses oneself to set up with optimization carries out model prediction to the liquid sample that second step gathers, and contrasts with its chemical measurements, requires that error is less than 10%.
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